CN110931386A - Method for manufacturing semiconductor device, substrate processing apparatus, and storage medium - Google Patents

Method for manufacturing semiconductor device, substrate processing apparatus, and storage medium Download PDF

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Publication number
CN110931386A
CN110931386A CN201910803231.9A CN201910803231A CN110931386A CN 110931386 A CN110931386 A CN 110931386A CN 201910803231 A CN201910803231 A CN 201910803231A CN 110931386 A CN110931386 A CN 110931386A
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gas
supply unit
supply
processing chamber
substrate
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CN201910803231.9A
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CN110931386B (en
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江端慎也
平松宏朗
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Kokusai Electric Corp
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Kokusai Electric Corp
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    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
    • H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
    • H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
    • H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
    • H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
    • C23C16/45546—Atomic layer deposition [ALD] characterized by the apparatus specially adapted for a substrate stack in the ALD reactor
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563—Gas nozzles
    • C23C16/45578—Elongated nozzles, tubes with holes
    • H—ELECTRICITY
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/0217—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon nitride not containing oxygen, e.g. SixNy or SixByNz
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
    • H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
    • H01L21/02211—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound being a silane, e.g. disilane, methylsilane or chlorosilane
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
    • H01L21/02299—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment
    • H01L21/02312—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment treatment by exposure to a gas or vapour
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
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    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67242—Apparatus for monitoring, sorting or marking
    • H01L21/67276—Production flow monitoring, e.g. for increasing throughput

Abstract

The invention provides a method for manufacturing a semiconductor device, a substrate processing apparatus, and a storage medium, which can improve the uniformity of the film quality in a substrate surface of a film formed on a substrate. A method for manufacturing a semiconductor device includes a step of forming a film on a substrate by performing a predetermined number of cycles, wherein (a) a step of supplying a source gas from a first supply unit to the substrate in a processing chamber and (b) a step of supplying a reaction gas from a second supply unit to the substrate in the processing chamber are performed non-simultaneously, and in (a), the source gas is decomposed in the first supply unit and the processing chamber to generate an intermediate, and the intermediate is supplied to the substrate, and at this time, the amount of decomposition of the source gas in the first supply unit is made larger than the amount of decomposition of the source gas in the processing chamber.

Description

Method for manufacturing semiconductor device, substrate processing apparatus, and storage medium
Technical Field
The invention relates to a method for manufacturing a semiconductor device, a substrate processing apparatus, and a storage medium.
Background
As one of the manufacturing processes of a semiconductor device, there is a case where a substrate processing step is performed in which a raw material gas and a reaction gas are supplied to a substrate in a processing chamber to form a film on the substrate (for example, see patent document 1).
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. 2012-33874
Disclosure of Invention
Problems to be solved by the invention
The purpose of the present invention is to provide a technique capable of improving the uniformity of the film quality in the substrate surface of a film formed on a substrate.
Means for solving the problems
According to an aspect of the present invention, the following technique is provided:
there is a step of forming a film on a substrate by performing cycles for a predetermined number of times,
the above cycles are performed non-simultaneously:
(a) supplying a source gas from a first supply unit to the substrate in the processing chamber; and
(b) supplying a reaction gas from a second supply unit to the substrate in the processing chamber,
in the step (a), the raw material gas is decomposed in the first supply unit and the processing chamber to generate an intermediate, and the intermediate is supplied to the substrate, and in this case, the decomposition amount of the raw material gas in the first supply unit is set to be larger than the decomposition amount of the raw material gas in the processing chamber.
Effects of the invention
According to the present invention, the uniformity of the film quality in the substrate surface of the film formed on the substrate can be improved.
Drawings
Fig. 1 is a schematic configuration diagram of a vertical processing furnace to which a substrate processing apparatus according to an embodiment of the present invention is applied, and is a diagram showing a portion of the processing furnace in a vertical cross-sectional view.
Fig. 2 is a schematic configuration diagram of a vertical processing furnace to which a substrate processing apparatus according to an embodiment of the present invention is applied, and is a diagram showing a portion of the processing furnace in a sectional view along line a-a of fig. 1.
Fig. 3 is a schematic configuration diagram of a controller applied to a substrate processing apparatus according to an embodiment of the present invention, and is a diagram showing a control system of the controller in a block diagram.
Fig. 4 is a diagram showing a film formation sequence according to the first embodiment of the present invention.
Fig. 5 is a diagram showing a film formation sequence according to a second embodiment of the present invention.
Fig. 6(a) is a schematic configuration diagram of first to third nozzles applied to first and second embodiments of the present invention, and (b) is a schematic configuration diagram of first to third nozzles applied to another embodiment of the present invention.
Fig. 7(a) and (b) are schematic structural views of a vertical processing furnace to which a substrate processing apparatus according to another embodiment of the present invention is applied.
Fig. 8 is a graph showing the evaluation results of the substrate in-plane refractive index uniformity and the substrate in-plane film thickness uniformity of the film formed on the substrate.
Detailed Description
< first embodiment >
The first embodiment will be described below with reference to fig. 1 to 4, fig. 6(a), and the like.
(1) Structure of substrate processing apparatus
As shown in fig. 1, the processing furnace 202 has a heater 207 as a heating means (temperature adjustment unit). The heater 207 has a cylindrical shape and is vertically installed by being supported by a holding plate. The heater 207 also functions as an activation mechanism (excitation unit) that activates (excites) the gas by heat. The heater 207 also functions as a decomposition unit for decomposing the source gas in the nozzle 249a serving as a first supply unit and the processing chamber 201, respectively, which will be described later.
The reaction tube 203 is disposed concentrically with the heater 207 inside the heater 207. The reaction tube 203 is made of, for example, quartz (SiO)2) Or a heat-resistant material such as silicon carbide (SiC), and is formed into a cylindrical shape having a closed upper end and an open lower end. A manifold 209 is disposed below the reaction tube 203 concentrically with the reaction tube 203. A manifold 209 is composed ofFor example, a metal material such as stainless steel (SUS) is formed in a cylindrical shape with an open upper end and a lower end. The upper end of the manifold 209 is engaged with the lower end of the reaction tube 203, and supports the reaction tube 203. An O-ring 220a as a sealing member is provided between the manifold 209 and the reaction tube 203. The reaction tube 203 is vertically installed in the same manner as the heater 207. The reaction tube 203 and the manifold 209 mainly constitute a processing container (reaction container). A processing chamber 201 is formed in a hollow portion of the processing container. The processing chamber 201 is configured to accommodate a wafer 200 as a substrate. The wafer 200 is processed in the processing chamber 201.
Nozzles 249a to 249c as first to third supply portions are provided in the processing chamber 201 so as to penetrate the side wall of the manifold 209. The nozzles 249a to 249c are made of a heat-resistant material such as quartz or SiC. The nozzles 249a to 249c are also referred to as first to third nozzles. Gas supply pipes 232a to 232c are connected to the nozzles 249a to 249c, respectively. The nozzles 249a to 249c are different nozzles, and the nozzles 249b and 249c are provided adjacent to the nozzle 249a, respectively, and are arranged so as to sandwich the nozzle 249a from both sides.
Mass Flow Controllers (MFCs) 241a to 241c as flow rate controllers (flow rate control units) and valves 243a to 243c as opening and closing valves are provided in this order from the upstream side of the gas flow in the gas supply pipes 232a to 232 c. A gas supply pipe 232d is connected to the gas supply pipe 232a on the downstream side of the valve 243 a. A gas supply pipe 232e is connected to the gas supply pipe 232b on the downstream side of the valve 243 b. The gas supply pipes 232d and 232e are provided with MFCs 241d and 241e and valves 243d and 243e, respectively, in this order from the upstream side of the gas flow. The gas supply pipes 232a to 232e are made of a metal material such as SUS, for example.
As shown in fig. 2, the nozzles 249a to 249c are provided along the inner wall of the reaction tube 203 from the lower portion to the upper portion, that is, along the wafer arrangement direction, in a space having an annular shape in plan view between the inner wall of the reaction tube 203 and the wafer 200. That is, the nozzles 249a to 249c are arranged along the wafer arrangement region in a region horizontally surrounding the wafer arrangement region on a side of the space (hereinafter, referred to as the wafer arrangement region) in which the wafers 200 are arranged. The nozzle 249a is disposed so as to be aligned with an exhaust port 231a described later across the center of the wafer 200 loaded into the processing chamber 201 in a plan view. The nozzles 249b and 249c are disposed adjacent to the nozzle 249a with a straight line passing through the nozzle 249a and the exhaust port 231a interposed therebetween. In other words, the nozzles 249b and 249c are arranged on both sides of the nozzle 249a, that is, along the inner wall of the reaction tube 203 (the outer peripheral portion of the wafer 200), the nozzle 249a is sandwiched from both sides.
As shown in fig. 6 a, each of the nozzles 249a to 249c is configured as a U-shaped nozzle (U-turn nozzle or return nozzle) having a bent portion (bent portion) in an inverted U-shape at the top of the nozzles 249a to 249c, i.e., above the upper end of the wafer alignment region. Gas ejection ports 250a to 250c for supplying (ejecting) gas are arranged along the wafer arrangement direction on the side surfaces of the nozzles 249a to 249 c. A plurality of gas ejection ports 250a to 250c are arranged from one end side to the other end side in the wafer arrangement direction in the wafer arrangement region. The gas ejection ports 250a to 250c are opened so as to face the exhaust port 231a in a plan view, and can supply gas toward the wafer 200. The gas ejection ports 250a to 250c are circular in shape when viewed from the wafer arrangement region side. The opening areas (apertures) of the gas ejection ports 250a to 250c are equal in size from one end side to the other end side in the wafer arrangement direction in the wafer arrangement region. The opening area (aperture) of the gas ejection port 250a is equal to or smaller than the opening area (aperture) of the gas ejection port 250b, and equal to or smaller than the opening area (aperture) of the gas ejection port 250 c.
As a raw material (source gas), for example, a halogenated silane gas containing silicon (Si) as a main element constituting a film to be formed and a halogen element is supplied from a gas supply pipe 232a into the processing chamber 201 through an MFC241a, a valve 243a, and a nozzle 249 a. The raw material gas is a gaseous raw material, and for example, a gas obtained by gasifying a raw material in a liquid state at normal temperature and normal pressure, a raw material in a gaseous state at normal temperature and normal pressure, or the like. The halosilane-based gas is a silane-based gas having a halogen group. The halogen group includes halogen elements such as chlorine (Cl), fluorine (F), bromine (Br), iodine (I) and the like. As the halosilane-based gas, for example, a chlorosilane-based gas, which is a raw material gas containing Si and Cl, can be used. The chlorosilane-based gas functions as an Si source. As chlorosilanesGas, for example, dichlorosilane (SiH) can be used2Cl2For short: DCS) gas.
As a reactant (reaction gas), for example, a gas containing nitrogen (N) is supplied from the gas supply pipe 232b into the processing chamber 201 through the MFC241b, the valve 243b, and the nozzle 249 b. The gas containing N functions as a nitriding source (nitriding agent, nitriding gas), that is, an N source. As the gas containing N, for example, ammonia (NH) as a hydrogen nitride-based gas can be used3) A gas.
As inert gases, e.g. nitrogen (N)2) The gas is supplied from the gas supply pipes 232d and 232e into the processing chamber 201 through the MFCs 241d and 241e, the valves 243d and 243e, the gas supply pipes 232a and 232b, and the nozzles 249a and 249b, respectively. In addition, as inert gas, for example, N2The gas is supplied from the gas supply pipe 232c into the processing chamber 201 through the MFC241c, the valve 243c, and the nozzle 249c, respectively. N is a radical of2The gas functions as a pressure adjusting gas for adjusting the pressure in the nozzles 249a to 249c, and also functions as a purge gas, a carrier gas, and a diluent gas.
The raw material gas supply system is mainly constituted by the gas supply pipe 232a, the MFC241a, and the valve 243 a. The reaction gas supply system is mainly constituted by the gas supply pipe 232b, the MFC241b, and the valve 243 b. The inert gas supply system is mainly constituted by gas supply pipes 232d, 232e, and 232c, MFCs 241d, 241e, and 241c, and valves 243d, 243e, and 243 c.
The decomposition amount of the raw material gas in the nozzle 249a is controlled not only by the temperature in the nozzle 249a but also by the pressure in the nozzle 249 a. The pressure in the nozzle 249a is affected by the opening area (aperture) of the gas ejection port 250a provided in the nozzle 249a, and therefore the nozzle 249a and the gas ejection port 250a can be included in the decomposition unit. Further, since the pressure in the nozzle 249a is affected by the flow rates of the raw material gas and the inert gas supplied into the nozzle 249a, it is also possible to include a raw material gas supply system for controlling the supply of the raw material gas into the nozzle 249a and an inert gas supply system for controlling the supply of the inert gas into the nozzle 249a in the decomposition unit.
Any one or all of the various supply systems described above may be configured as an integrated supply system 248 including the cluster valves 243a to 243e, the MFCs 241a to 241e, and the like. The integrated supply system 248 is connected to each of the gas supply pipes 232a to 232e, and controls supply operations of various gases to the gas supply pipes 232a to 232e, that is, opening and closing operations of the valves 243a to 243e, flow rate adjustment operations by the MFCs 241a to 241e, and the like, by the controller 121 described later. The integrated supply system 248 is configured as an integrated unit or a divided integrated unit, is detachable from the gas supply pipes 232a to 232e and the like in the integrated unit, and is configured such that maintenance, replacement, addition and the like of the integrated supply system 248 can be performed in the integrated unit.
An exhaust port 231a for exhausting the gas medium in the processing chamber 201 is provided below the side wall of the reaction tube 203. As shown in fig. 2, the exhaust port 231a is provided at a position facing (facing) the nozzles 249a to 249c (gas ejection ports 250a to 250c) through the wafer 200 in a plan view. The exhaust port 231a may be provided along the wafer arrangement region from the lower portion to the upper portion of the sidewall of the reaction tube 203. An exhaust pipe 231 is connected to the exhaust port 231 a. A vacuum pump 246 as a vacuum pumping device is connected to the exhaust pipe 231 via a Pressure sensor 245 as a Pressure detector (Pressure detecting unit) for detecting the Pressure in the processing chamber 201 and an apc (auto Pressure controller) valve 244 as a Pressure regulator (Pressure adjusting unit). The APC valve 244 is configured to be opened and closed in a state where the vacuum pump 246 is operated, thereby enabling evacuation and stop of evacuation in the processing chamber 201, and to be opened and closed in a state where the vacuum pump 246 is operated, thereby adjusting the opening of the valve based on the pressure information detected by the pressure sensor 245, thereby enabling adjustment of the pressure in the processing chamber 201. The exhaust pipe 231, the APC valve 244, and the pressure sensor 245 mainly constitute an exhaust system. It is also contemplated that the vacuum pump 246 may be included in the exhaust system. The decomposition amount of the source gas in the processing chamber 201 is controlled not only by the temperature in the processing chamber 201 but also by the pressure in the processing chamber 201. Therefore, the APC valve 244 can be included in the decomposition unit.
A seal cap 219 serving as a furnace opening lid body that can hermetically close the lower end opening of the manifold 209 is provided below the manifold 209. The seal cap 219 is made of a metal material such as SUS, and is formed in a disk shape. An O-ring 220b as a sealing member abutting against the lower end of the manifold 209 is provided on the upper surface of the seal cap 219. A rotation mechanism 267 for rotating the boat 217 described later is provided below the seal cap 219. The rotary shaft 255 of the rotary mechanism 267 penetrates the seal cover 219 and is connected to the boat 217. The rotation mechanism 267 is configured to rotate the wafer 200 by rotating the boat 217. The sealing cap 219 is configured to be vertically lifted by the boat elevator 115 as a lifting mechanism provided outside the reaction tube 203. The boat elevator 115 is configured as a conveying device (conveying mechanism) that moves the wafer 200 into and out of the processing chamber 201 by moving the seal cap 219 up and down. A shutter 219s is provided below the manifold 209, and the shutter 219s functions as a furnace opening lid body capable of hermetically closing the lower end opening of the manifold 209 in a state where the seal cap 219 is lowered and the boat 217 is carried out from the processing chamber 201. The shutter 219s is formed of a metal material such as SUS, and is formed in a disk shape. An O-ring 220c as a sealing member abutting against the lower end of the manifold 209 is provided on the upper surface of the shutter 219 s. The opening and closing operation (the lifting operation, the turning operation, and the like) of the shutter 219s is controlled by the shutter opening and closing mechanism 115 s.
The boat 217 serving as a substrate support portion is configured to support a plurality of wafers 200, for example, 25 to 200 wafers, in a horizontal posture and in a state of being aligned with each other at the center, in a vertical direction, in a multi-stage manner, that is, in a spaced-apart manner. The boat 217 is made of a heat-resistant material such as quartz or SiC. A plurality of heat insulating plates 218 made of a heat-resistant material such as quartz or SiC are supported on the lower portion of the boat 217.
A temperature sensor 263 as a temperature detector is provided in the reaction tube 203. By adjusting the state of energization to the heater 207 based on the temperature information detected by the temperature sensor 263, the temperature in the processing chamber 201 becomes a desired temperature distribution. The temperature sensor 263 is disposed along the inner wall of the reaction tube 203.
As shown in fig. 3, the controller 121 as a control unit (control means) is configured as a computer including a cpu (central processing unit)121a, a RAM (Random Access Memory)121b, a storage device 121c, and an I/O port 121 d. The RAM121b, the storage device 121c, and the I/O port 121d are configured to be capable of exchanging data with the CPU121a via the internal bus 121 e. An input/output device 122 configured as, for example, a touch panel or the like is connected to the controller 121.
The storage device 121c is configured by, for example, a flash memory, an hdd (hard Disk drive), or the like. The storage device 121c stores a control program for controlling the operation of the substrate processing apparatus, a process recipe in which steps, conditions, and the like of substrate processing described later are described so as to be readable. The process recipe is a combination of steps in substrate processing described later so that a predetermined result can be obtained by the controller 121, and functions as a program. Hereinafter, the process recipe, the control program, and the like are collectively referred to as simply a program. In addition, the process recipe is also simply referred to as a recipe. The term "program" as used in this specification sometimes includes only recipe monomers, sometimes only control program monomers, or both. The RAM121b is configured as a storage area (work area) that temporarily holds programs, data, and the like read by the CPU121 a.
The I/O port 121d is connected to the MFCs 241a to 241e, the valves 243a to 243e, the pressure sensor 245, the APC valve 244, the vacuum pump 246, the temperature sensor 263, the heater 207, the rotation mechanism 267, the boat elevator 115, the shutter opening/closing mechanism 115s, and the like.
The CPU121a is configured to read out and execute a control program from the storage device 121c, and read out a recipe from the storage device 121c in accordance with input of an operation instruction from the input/output device 122, and the like. The CPU121a is configured to control the flow rate adjustment operation of the MFCs 241a to 241e for each gas, the opening and closing operation of the valves 243a to 243e, the opening and closing operation of the APC valve 244, the pressure adjustment operation of the APC valve 244 by the pressure sensor 245, the start and stop of the vacuum pump 246, the temperature adjustment operation of the heater 207 by the temperature sensor 263, the rotation and rotation speed adjustment operation of the boat 217 by the rotation mechanism 267, the lifting and lowering operation of the boat 217 by the boat lifter 115, the opening and closing operation of the shutter 219s by the shutter opening and closing mechanism 115s, and the like, in accordance with the content of the read recipe.
The controller 121 can be configured by installing the program stored in the external storage device 123 in a computer. The external storage device 123 includes, for example, a magnetic disk such as an HDD, an optical disk such as a CD, an optical magnetic disk such as an MO, a semiconductor memory such as a USB memory, and the like. The storage device 121c and the external storage device 123 are configured as computer-readable storage media. Hereinafter, they will be collectively referred to simply as storage media. In the present specification, the term "storage medium" may be used to include only the storage device 121c alone, only the external storage device 123 alone, or both of them. Further, the program may be provided to the computer by a communication method such as the internet or a dedicated line without using the external storage device 123.
(2) Substrate processing procedure
A substrate processing sequence example, i.e., a film sequence example, in which a film is formed on a wafer 200 as a substrate, will be described using the substrate processing apparatus as one step of a manufacturing process of a semiconductor device, with reference to fig. 4. In the following description, the operations of the respective parts constituting the substrate processing apparatus are controlled by the controller 121.
In the film formation sequence shown in fig. 4, a silicon nitride film (SiN film) as a film containing Si and N is formed on the wafer 200 as a film by performing the following cycles a predetermined number of times (N times, N being an integer of 1 or more), the cycles being performed non-simultaneously:
a step a of supplying DCS gas as a source gas from a nozzle 249a as a first supply unit to the wafer 200 in the process chamber 201; and
reacting NH3And B, supplying the gas as a reaction gas from a nozzle 249B as a second supply unit to the wafer 200 in the process chamber 201.
In addition, when the film formation sequence shown in fig. 4 is performed, in step a, the intermediate product is generated by decomposing the DCS gas in the nozzle 249a and the process chamber 201, and is supplied to the wafer 200, in which case the decomposition amount of the DCS gas in the nozzle 249a is set to be larger than the decomposition amount of the DCS gas in the process chamber 201.
In fig. 4, the implementation periods of step A, B are respectively denoted as A, B for convenience of explanation. In the present specification and fig. 4, for convenience of description, the nozzles 249a to 249c are also denoted by R1 to R3, respectively. The period of execution of each step and the reference numerals of each nozzle are the same in fig. 5 showing the gas supply sequence of other embodiments described later.
In this specification, for convenience of explanation, the film formation sequence shown in fig. 4 is sometimes shown as follows. In the description of other embodiments to be described later, the same reference numerals are used.
Figure BDA0002182909050000081
The term "wafer" used in the present specification may refer to the wafer itself, or a laminate of the wafer and a predetermined layer or film formed on the surface thereof. The term "surface of wafer" used in the present specification may refer to a surface of a wafer itself, or may refer to a surface of a predetermined layer or the like formed on a wafer. In the present specification, the case where "a predetermined layer is formed on a wafer" is described, in some cases, where the predetermined layer is formed directly on the surface of the wafer itself, or where the predetermined layer is formed on a layer or the like formed on the wafer. The term "substrate" used in the present specification is also the same as the term "wafer".
(wafer Loading and boat Loading)
The wafer boat 217 is loaded with a plurality of wafers 200. Thereafter, as shown in fig. 1, the boat 217 holding the plurality of wafers 200 is lifted by the boat elevator 115 and carried into the process chamber 201 (boat loading). In this state, the sealing cap 219 is in a state of sealing the lower end of the manifold 209 via the O-ring 220 b.
(pressure adjustment and temperature adjustment)
The processing chamber 201, i.e., the space in which the wafer 200 is present, is evacuated (depressurized and exhausted) by a vacuum pump 246 to a desired pressure (processing pressure). At this time, the pressure in the processing chamber 201 is measured by the pressure sensor 245, and the APC valve 244 is feedback-controlled based on the measured pressure information. The wafer 200 in the processing chamber 201 is heated by the heater 207 to a desired temperature (processing temperature). At this time, the energization state of the heater 207 is feedback-controlled based on the temperature information detected by the temperature sensor 263 so that the inside of the processing chamber 201 has a desired temperature distribution. Further, the rotation of the wafer 200 by the rotation mechanism 267 is started. The evacuation of the processing chamber 201, the heating of the wafer 200, and the rotation are continued at least until the end of the processing of the wafer 200.
(film Forming step)
Thereafter, the next step A, B is performed in sequence.
[ step A ]
In this step, DCS gas is supplied to the wafer 200 in the process chamber 201 (DCS gas supply step). Specifically, the valve 243a is opened to flow the DCS gas into the gas supply pipe 232 a. The DCS gas is flow-rate-adjusted by the MFC241a, supplied into the process chamber 201 through each of the plurality of gas outlets 250a provided on the side surface of the nozzle 249a, and discharged from the exhaust port 231 a. At this time, the valves 243d, 243e, and 243c are opened to supply N into the processing chamber 201 through the nozzles 249a to 249c2A gas. N supplied from each of the nozzles 249a to 249c2The flow rate of the gas is equal to or less than the flow rate of the DCS gas supplied from the nozzle 249 a. Further, N from the nozzles 249a to 249c into the processing chamber 201 may not be performed2And (3) supplying gas.
The processing conditions in this step are shown as examples:
DCS gas supply flow rate: 0.001 to 3slm, preferably 0.01 to 1.5slm
N2Gas supply flow rate (each of R1 to R3): 0 to 3slm, preferably 0 to 1.5slm
Supply time of each gas: 1 to 300 seconds, preferably 2 to 120 seconds, and more preferably 5 to 60 seconds
Treatment temperature: 500 to 850 ℃, preferably 550 to 700 DEG C
Treatment pressure: 1 to 4666Pa, preferably 133 to 3999Pa
In the present specification, the numerical range of "500 to 850 ℃ means that the lower limit value and the upper limit value are included in the range. Thus, for example, "500 to 850 ℃ means" 500 ℃ to 850 ℃. The same applies to other numerical ranges.
In the DCS gas supply step, DCS gas can be thermally decomposed in the nozzle 249a and the process chamber 201, respectively, to generate a Substance (SiH) obtained by partial decomposition of DCSxCly) I.e. an intermediate.
In the present embodiment, the decomposition rate (decomposition rate) of the DCS gas in the nozzle 249a is set to be higher than the decomposition rate (decomposition rate) of the DCS gas in the process chamber 201. That is, the decomposition amount of the DCS gas in the nozzle 249a is set to be larger than the decomposition amount of the DCS gas in the process chamber 201. In other words, the rate of production (production rate) of the intermediate in the nozzle 249a is set to be greater than the rate of production (production rate) of the intermediate in the processing chamber 201. That is, the amount of the intermediate produced in the nozzle 249a is set to be larger than the amount of the intermediate produced in the processing chamber 201.
The amount of DCS gas decomposition, i.e., the amount of generated intermediates, in the nozzle 249a tends to increase as the pressure in the nozzle 249a increases. In the present embodiment, the opening area (aperture) of the gas ejection port 250a is set to be equal to or smaller than the opening area (aperture) of the gas ejection port 250b, and preferably, the opening area (aperture) of the gas ejection port 250a is set to be equal to or smaller than the opening area (aperture) of the gas ejection port 250b and equal to or smaller than the opening area (aperture) of the gas ejection port 250c, so that the pressure in the nozzle 249a can be appropriately increased when the nozzle 249a is used under the above-described process conditions. Further, by making the opening area (aperture) of the gas ejection port 250a smaller than the opening area (aperture) of the gas ejection port 250b, it is preferable that the opening area (aperture) of the gas ejection port 250a is smaller than the opening area (aperture) of the gas ejection port 250b and smaller than the opening area (aperture) of the gas ejection port 250c, and therefore, when the nozzle 249a is used under the above-described process conditions, the pressure in the nozzle 249a can be further appropriately increased. In any of these cases, the pressure in the nozzle 249a can be made higher than the pressure in the processing chamber 201, and an appropriate pressure difference can be provided between the inside of the nozzle 249a and the inside of the processing chamber 201. This allows a CVD reaction to occur in the nozzle 249a, thereby promoting decomposition of DCS gas in the nozzle 249a, i.e., formation of intermediates, and bringing the above state into effect. The opening area (aperture) of the gas discharge port 250a provided in the nozzle 249a may be an opening area (aperture) that allows the amount of decomposition, the decomposition rate, and the decomposition rate of DCS gas (the amount of intermediate produced, the production rate, and the production rate) to be at least one of the above states in the nozzle 249a in the DCS gas supply step.
By supplying DCS gas containing the intermediate to the wafer 200, a Si-containing layer containing Cl is formed on the outermost surface of the wafer 200. The Si-containing layer containing Cl is formed by physically adsorbing DCS, chemisorption, deposition of intermediates, thermal decomposition of DCS and intermediates, deposition of Si, and the like on the outermost surface of the wafer 200. The Si layer containing Cl may include DCS, an adsorption layer of an intermediate (physisorption layer, chemisorption layer), a deposition layer of an intermediate, or a Si layer containing Cl (deposition layer of Si). In this specification, the Si-containing layer containing Cl is simply referred to as a Si-containing layer.
In the DCS gas supply step, the pressure in the process chamber 201 is preferably set to NH in step B, which will be described later3The pressure in the processing chamber 201 in the gas supply step is preferably higher than the pressure in NH in step B3The pressure in the processing chamber 201 in the gas supply step is large.
After the Si-containing layer is formed, the valve 243a is closed to stop the supply of the DCS gas into the process chamber 201. Then, the inside of the processing chamber 201 is evacuated to remove the gas and the like remaining in the processing chamber 201 from the inside of the processing chamber 201 (purge step). At this time, N is supplied from the nozzles 249a to 249c into the processing chamber 2012A gas. N is a radical of2The gas acts as a purge gas.
As the raw material gas, monochlorosilane (SiH) can be used in addition to DCS gas3Cl, abbreviation: MCS) gas, trichlorosilane (SiHCl)3For short: TCS) gas, tetrachlorosilane (SiCl)4For short: STC) gas, hexachlorodisilane (Si)2Cl6For short: HCDS) gas, octachlorotris silane (Si)3Cl8For short: OCTS) gas, and the like. This point is the same as in other embodiments described laterAnd (5) sampling.
As inert gas, except for N2As the gas, a rare gas such as Ar gas, He gas, Ne gas, or Xe gas can be used. This is the same in step B and other embodiments described later.
[ step B ]
After step A is completed, NH is supplied to the wafer 200 in the processing chamber 201, that is, the Si-containing layer formed on the wafer 2003Gas (NH)3Gas supply step). Specifically, valve 243b is opened to allow NH3The gas flows into the gas supply pipe 232 b. NH (NH)3The gas is supplied into the processing chamber 201 through each of the plurality of gas ejection ports 250b provided on the side surface of the nozzle 249b while being flow-adjusted by the MFC241b, and is discharged from the exhaust port 231 a. At this time, NH is supplied to the wafer 2003A gas. At this time, at least one of the valves 243d, 243e, and 243c may be opened to supply N into the processing chamber 201 through at least one of the nozzles 249a to 249c2A gas.
The processing conditions in this step are shown as examples:
NH3gas supply flow rate: 1-20 slm
N2Gas supply flow rate (each of R1 to R3): 0 to 5slm
NH3Gas supply time: 1 to 120 seconds, preferably 1 to 60 seconds
Treatment pressure: 1 to 3999Pa, preferably 67 to 2666 Pa.
The other processing conditions were the same as those in step A.
By supplying NH to the wafer 200 under the above-described conditions3The gas, at least a portion of the Si-containing layer formed on the wafer 200 is nitrided (modified). By modifying the Si-containing layer, a SiN layer, which is a layer containing Si and N, is formed on the wafer 200. In the formation of the SiN layer, impurities such as Cl contained in the Si-containing layer are present in NH3During the modification reaction of the Si-containing layer with the gas, a gaseous substance containing at least Cl is formed and discharged from the processing chamber 201. Thus, the SiN layer becomes a layer containing less impurities such as Cl than the Si-containing layer.
After the SiN layer is formed, the valve 243b is closed to stop the flow into the processing chamber 20NH within 13And (3) supplying gas. Then, the gas and the like remaining in the processing chamber 201 are exhausted from the processing chamber 201 through the same processing steps as the purge step of step a (purge step).
As reaction gas, except NH3Gas, it is also possible to use, for example, hydrazine (N)2H2) Gas, hydrazine (N)2H4) Gas, N3H8A hydrogen nitride-based gas such as a gas. This point is also the same in other embodiments described later.
[ predetermined number of executions ]
By performing the cycle of step A, B described above a predetermined number of times (n times, n being an integer of 1 or more) non-simultaneously, i.e., asynchronously, SiN films of a predetermined composition and a predetermined film thickness can be formed on wafer 200. The above cycle is preferably repeated a plurality of times. That is, the SiN layer formed by performing the above-described cycle once is preferably made thinner than a desired film thickness, and the above-described cycle is preferably repeated a plurality of times until the film thickness of the SiN layer formed by stacking the SiN layers becomes the desired film thickness.
(post-purification-atmospheric pressure recovery)
After the film formation step is completed, N is supplied from each of the nozzles 249a to 249c into the processing chamber 2012The gas is exhausted from the exhaust pipe 231 through the exhaust port 231 a. N is a radical of2The gas acts as a purge gas. Thereby, the inside of the processing chamber 201 is purged, and the gas and reaction by-products remaining in the processing chamber 201 are removed from the inside of the processing chamber 201 (post-purge). Thereafter, the gas medium in the processing chamber 201 is replaced with an inert gas (inert gas replacement), and the pressure in the processing chamber 201 is returned to the normal pressure (atmospheric pressure recovery).
(wafer unloading and wafer unloading)
The sealing cap 219 descends by the boat elevator 115, and the lower end of the manifold 209 is opened. Then, the processed wafer 200 is carried out from the lower end of the manifold 209 to the outside of the reaction tube 203 while being supported by the boat 217 (boat unloading). The processed wafer 200 is carried out to the outside of the reaction tube 203 and then taken out from the boat 217 (wafer unloading).
(3) Effects of the present embodiment
According to the present embodiment, one or more of the following effects can be obtained.
(a) In the DCS gas supply step of step a, by appropriately increasing the pressure in the nozzle 249a under the above-described process conditions, an appropriate pressure difference can be provided between the inside of the nozzle 249a and the inside of the process chamber 201, and a state can be achieved in which the amount of decomposition of DCS gas (amount of generated intermediate) in the nozzle 249a is greater than the amount of decomposition of DCS gas (amount of generated intermediate) in the process chamber 201. As a result, the uniformity of the in-plane refractive index of the SiN film formed on the wafer 200 (hereinafter referred to as in-plane refractive index uniformity) can be improved. This is considered to be because the wafer in-plane composition ratio uniformity (hereinafter referred to as in-plane composition ratio uniformity) of the SiN film formed on the wafer 200 can be improved by controlling the decomposition amount of DCS gas (the amount of generated intermediate) as described above.
That is, in the conventional film formation method, the intermediate may not reach the center of the wafer 200, and thus the ratio of Si to N in the SiN film in the center of the wafer 200 may be lower than the ratio of Si to N in the SiN film in the outer periphery of the wafer 200. In contrast, according to the present embodiment, by providing an appropriate pressure difference between the inside of the nozzle 249a and the inside of the process chamber 201 and controlling the amount of decomposition of DCS gas (the amount of intermediate product generated) as described above, the intermediate product can be efficiently brought to the central portion as well as the outer peripheral portion of the wafer 200. This makes it possible to equalize the ratio of Si to N of the SiN film formed on the wafer 200 between the outer peripheral portion and the central portion of the wafer 200, and to make the composition ratio of the SiN film formed on the wafer 200 uniform over the entire wafer surface. According to the present embodiment, for example, when forming a Si-rich SiN film on the wafer 200, the SiN film formed on the wafer 200 can be made to be a Si-rich film over the entire wafer surface by making the SiN film at the center portion Si-rich as well as the SiN film at the outer periphery of the wafer 200.
(b) The opening area (aperture) of the gas ejection port 250a of the nozzle 249a for supplying the raw material gas is preferably equal to or smaller than the opening area (aperture) of the gas ejection port 250b of the nozzle 249b for supplying the reaction gas. By setting the opening area (aperture) of the gas ejection port 250a to be equal to or smaller than the opening area (aperture) of the gas ejection port 250b, the pressure in the nozzle 249a in the DCS gas supply step can be reliably increased, and the above-described effects can be reliably obtained. Further, it is more preferable that the opening area (aperture) of the gas ejection port 250a of the nozzle 249a for supplying the raw material gas is smaller than the opening area (aperture) of the gas ejection port 250b of the nozzle 249b for supplying the reaction gas. By making the opening area (aperture diameter) of the gas ejection port 250a smaller than the opening area (aperture diameter) of the gas ejection port 250b, the pressure in the nozzle 249a in the DCS gas supply step can be increased more reliably, and the above-described effects can be obtained more reliably.
(c) The opening area (aperture) of the gas ejection port 250a of the nozzle 249a for supplying the raw material gas is preferably set to be equal to or smaller than the opening area (aperture) of the gas ejection ports 250b and 250c of the nozzles 249b and 249c for supplying other gases (reaction gas and inert gas). By setting the opening area (aperture) of the gas ejection port 250a to be equal to or smaller than the opening area (aperture) of the gas ejection port 250b and equal to or smaller than the opening area (aperture) of the gas ejection port 250c, the pressure in the nozzle 249a in the DCS gas supply step can be reliably increased, and the above-described effects can be reliably obtained. Further, the opening area (aperture) of the gas ejection port 250a of the nozzle 249a for supplying the raw material gas is preferably smaller than the opening area (aperture) of the gas ejection ports 250b and 250c of the nozzles 249b and 249c for supplying other gases (reaction gas and inert gas). By making the opening area (aperture) of the gas ejection port 250a smaller than the opening area (aperture) of the gas ejection port 250b and smaller than the opening area (aperture) of the gas ejection port 250c, the pressure in the nozzle 249a in the DCS gas supply step can be more reliably increased, and the above-described effects can be more reliably obtained.
(d) Preferably, in the DCS gas supply step of step a, the pressure in the process chamber 201 is set to NH of step B3The pressure in the processing chamber 201 in the gas supply step (at least the pressure at which nitridation of the Si-containing layer is appropriately performed) is not less than. This can improve the appearance of the gap between the inner wall of the reaction tube 203 and the wafer 200 in plan viewSince the pressure in the annular space is low, the conductance in the space is reduced, and the flow of DCS gas containing the intermediate from the gap to the lower side is suppressed. This enables efficient supply of the intermediate to the center portion of the wafer 200, and as a result, uniformity of in-plane refractive index and uniformity of in-plane film thickness of the SiN film formed on the wafer 200 can be improved. In the DCS gas supply step of step A, the pressure in the processing chamber 201 is set to be higher than that of NH of step B3The pressure in the processing chamber 201 in the gas supply step (at least the pressure at which nitridation of the Si-containing layer is appropriately performed) is high, and the above-described effects can be obtained more reliably.
(e) According to this embodiment, a SiN film can be formed on the wafer 200, and the SiN film has good electrical properties and wafer in-plane film thickness uniformity (hereinafter referred to as in-plane film thickness uniformity), small surface roughness (surface smoothness), and excellent in-plane refractive index uniformity. In addition, according to the present embodiment, it is not necessary to enlarge the arrangement interval (pitch) of the wafers 200 in the wafer arrangement region in order to obtain these characteristics. Therefore, a decrease in productivity and an increase in cost in substrate processing can be avoided.
(f) The above-mentioned effects are obtained by using NH in the case where the above-mentioned raw material gas other than DCS gas is used3In the case of the above-mentioned reaction gas other than the gas, N is used2The same applies to the case of the above-mentioned inert gas other than the gas.
< second embodiment >
Hereinafter, a second embodiment will be described with reference to fig. 5.
In the present embodiment, as in the film formation sequence shown in fig. 5, in the DCS gas supply step of step a, N is supplied from the nozzle 249a to the wafer 2002Gas, N supplied from nozzle 249a2The flow rate of the gas is larger than the flow rate of the DCS gas supplied from the nozzle 249 a. Otherwise, the same as the first embodiment described above is applied.
The processing conditions in the DCS gas supply step in step a of the present embodiment are as follows:
DCS gas supply flow rate: 0.001 to 3slm, preferably 0.01 to 1.5slm
N2Gas supply flow rate (R1): 5 to 40slm, preferably 10 to 30slm
N2Gas supply flow rate (R2, R3): 0 to 3 slm.
The other processing conditions in step a are the same as those in step a of the first embodiment described above.
The processing procedure and processing conditions in step B are the same as those in step B of the first embodiment described above.
According to the present embodiment, in the DCS gas supply step, N supplied from the nozzle 249a is supplied2Gas, i.e. N acting as a pressure-regulating gas2The flow rate of the gas is larger than the flow rate of the DCS gas supplied from the nozzle 249a, so that the pressure in the nozzle 249a can be increased, and decomposition of the DCS gas in the nozzle 249a can be promoted. As a result, the amount of decomposition of DCS gas (amount of generated intermediate) in the nozzle 249a can be reliably made larger than the amount of decomposition of DCS gas (amount of generated intermediate) in the process chamber 201. This can reliably improve the in-plane refractive index uniformity of the SiN film formed on the wafer 200.
In addition, according to the present embodiment, in the DCS gas supply step, N supplied from the nozzle 249a is supplied2Gas, i.e. N acting as carrier gas2The flow rate of the gas is larger than the flow rate of the DCS gas supplied from the nozzle 249a, so that the DCS gas containing the intermediate flowing from the nozzle 249a can be pushed toward the wafer 200, thereby facilitating the supply of the intermediate to the center portion of the wafer 200. Further, due to this squeezing effect, the DCS gas containing the intermediate can be suppressed from flowing down through the gap between the inner wall of the reaction tube 203 and the wafer 200, and the intermediate can be efficiently supplied to the central portion of the wafer 200. Further, the pressure of the annular space in plan view in the gap between the inner wall of the reaction tube 203 and the wafer 200 can be increased, the conductance of the space can be reduced, and the flow of DCS gas containing the intermediate from the gap to the lower side can be further suppressed. This can more reliably improve the in-plane refractive index uniformity of the SiN film formed on the wafer 200. In addition, this makes it possible to more reliably perform the operationThe uniformity of the in-plane film thickness of the SiN film formed on the wafer 200 is improved.
In the DCS gas supply step, N supplied from a nozzle 249a is supplied2The flow rate of the gas is larger than the flow rate of the DCS gas supplied from the nozzle 249a and is larger than N supplied from each of the nozzles 249b and 249c2The above-described effects can be obtained more reliably by controlling the flow rate balance of each gas so that the flow rate of each gas is large.
In the DCS gas supply step, N supplied from the nozzle 249a is supplied2The flow rate of the gas is larger than the flow rate of the DCS gas supplied from the nozzle 249a and is larger than N supplied from each of the nozzles 249b and 249c2The above-described effects can be more reliably obtained by controlling the flow rate balance of each gas so that the total flow rate of the gases is large.
< Another embodiment >
The embodiments of the present invention have been specifically described above. However, the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the scope of the invention.
For example, as shown in fig. 6(b), as the nozzles 249a to 249c, long nozzles may be used which are configured to rise upward in the wafer arrangement direction from the lower portion to the upper portion of the inner wall of the reaction tube 203. In the nozzles 249a to 249c shown in fig. 6(b), a plurality of gas ejection ports 250a to 250c are also arranged from one end side to the other end side in the wafer arrangement direction in the wafer arrangement region, and the opening areas (apertures) of the respective ports are of uniform size. In this case, the opening area (aperture) of the gas ejection port 250a is not more than the opening area (aperture) of the gas ejection port 250b and not more than the opening area (aperture) of the gas ejection port 250 c. In this embodiment, the opening area (aperture) of the gas ejection port 250a is preferably smaller than the opening area (aperture) of the gas ejection port 250b, and more preferably smaller than the opening area (aperture) of the gas ejection port 250 c. In these cases, the same effects as those of the above-described embodiment can be obtained.
For example, two or more nozzles for supplying DCS gas may be provided, and in the DCS gas supply step, DCS gas may be supplied through the two or more nozzles. In this case, the same effects as those of the above-described embodiment can be obtained. Further, according to this embodiment, as compared with the case where the DCS gas is supplied through one nozzle, the amount of the DCS gas supplied can be doubled or more, and the amount of the intermediate supplied to the center portion of the wafer 200 can be doubled or more by 2, so that the effects obtained by the above-described embodiment can be improved.
For example, tris (dimethylamino) silane (SiH [ N (CH)) can be used as the raw material gas in addition to the chlorosilane-based gas3)2]3For short: 3DMAS) gas, bis (diethylamino) Silane (SiH)2[N(C2H5)2]2For short: BDEAS) gas, and the like. In this case, the same effects as those of the above-described embodiment can be obtained.
In addition, for example, propylene (C) can be used as the reaction gas3H6) Gas or the like carbon (C) -containing gas, triethylamine ((C)2H5)3N, abbreviation: n and C-containing gases such as TEA gas, and boron trichloride (BCl)3) Boron (B) -containing gas, oxygen (O), etc2) Gas, ozone (O)3) Gas, plasma excited O2Gas (O)2＊)、O2Gas + hydrogen (H)2) Gas, water vapor (H)2O gas), etc.
The present invention can also be applied to a case where a film containing Si such as a silicon oxynitride film (SiON film), a silicon oxycarbide film (SiOC film), a silicon carbonitride film (SiCN film), a silicon oxycarbonitride film (SiOCN film), a silicon boron nitride carbide film (SiBCN film), a silicon boron nitride film (SiBN film), or a silicon oxide film (SiO film) is formed on a substrate by the following film formation sequence. The process steps and process conditions for supplying the raw material gas and the reaction gas can be the same as those in the respective steps of the above-described embodiment, for example. In these cases, the same effects as those of the above-described embodiment can be obtained.
Figure BDA0002182909050000171
Figure BDA0002182909050000172
Figure BDA0002182909050000173
Figure BDA0002182909050000174
Figure BDA0002182909050000175
Figure BDA0002182909050000176
Figure BDA0002182909050000177
In addition, for example, titanium tetrachloride (TiCl) is used as the raw material4) Gas, trimethylaluminum (Al (CH)3)3For short: TMA) gas, etc., the present invention can be applied to a case where a film containing a metal element such as a titanium nitride film (TiN film), a titanium oxynitride film (TiON film), a titanium aluminum carbonitride film (TiAlCN film), a titanium aluminum carbide film (TiAlC film), a titanium carbonitride film (TiCN film), a titanium oxide film (TiO film) is formed on a substrate by the following film formation sequence. The process steps and process conditions for supplying the raw material gas and the reaction gas can be the same as those in the respective steps of the above-described embodiment, for example. In these cases, the same effects as those of the above-described embodiment can be obtained.
Figure BDA0002182909050000181
Figure BDA0002182909050000182
Figure BDA0002182909050000183
Figure BDA0002182909050000184
Figure BDA0002182909050000185
Figure BDA0002182909050000186
Preferably, recipes for substrate processing are prepared separately according to the contents of the processing and stored in the storage device 121c via the telecommunication line and the external storage device 123. Further, when starting the substrate processing, the CPU121a preferably selects an appropriate recipe from the plurality of recipes stored in the storage device 121c as appropriate according to the contents of the substrate processing. Thus, films of various types, component ratios, film qualities, and film thicknesses can be formed with good reproducibility by one substrate processing apparatus. In addition, the burden on the operator can be reduced, an operation error can be avoided, and the process can be started quickly.
The recipe is not limited to the case of being newly created, and may be prepared by changing an existing recipe already installed in the substrate processing apparatus, for example. In the case of changing the recipe, the recipe after the change may be installed in the substrate processing apparatus via a telecommunication line or a storage medium storing the recipe. Further, the input/output device 122 provided in the existing substrate processing apparatus may be operated to directly change the existing recipe installed in the substrate processing apparatus.
In the above-described embodiment, an example was described in which the first to third nozzles (nozzles 249a to 249c) as the first to third supply portions were provided in the processing chamber so as to extend along the inner wall of the reaction tube. However, the present invention is not limited to the above-described embodiments. For example, as shown in fig. 7(a), a cross-sectional structure of a vertical processing furnace may be employed, in which a buffer chamber is provided in a side wall of the reaction tube, and first to third nozzles having the same configuration as in the above-described embodiment are provided in the buffer chamber in the same arrangement as in the above-described embodiment. Fig. 7(a) shows an example in which a supply buffer chamber and an exhaust buffer chamber are provided in the side wall of the reaction tube, and are disposed at positions facing each other with the wafer interposed therebetween. The supply buffer chamber and the exhaust buffer chamber are provided along the sidewall of the reaction tube from the lower portion to the upper portion, that is, along the wafer alignment region. Fig. 7(a) shows an example in which the supply buffer chamber is partitioned into a plurality of (three) spaces, and each nozzle is disposed in each space. The arrangement of the three spaces of the buffer chamber is the same as the arrangement of the first to third nozzles. The spaces in which the first to third nozzles are disposed may be referred to as first to third buffer chambers. The first nozzle and the first buffer chamber, the second nozzle and the second buffer chamber, and the third nozzle and the third buffer chamber may be regarded as the first supply unit, the second supply unit, and the third supply unit, respectively. For example, as shown in fig. 7(b) which shows a cross-sectional structure of the vertical processing furnace, a buffer chamber may be provided in the same arrangement as in fig. 7(a), a first nozzle may be provided in the buffer chamber, and second and third nozzles may be provided along the inner wall of the reaction tube with a communicating portion with the processing chamber of the buffer chamber interposed therebetween. The first nozzle, the buffer chamber, the second nozzle, and the third nozzle may be considered as a first supply unit, a second supply unit, and a third supply unit, respectively. The structures of the buffer chamber and the reaction tube other than those described in fig. 7(a) and 7(b) are the same as those of the respective portions of the processing furnace shown in fig. 1. Even when these processing furnaces are used, the same substrate processing as in the above-described embodiment can be performed, and the same effects as in the above-described embodiment can be obtained.
In the above-described embodiments, an example of forming a film using a batch-type substrate processing apparatus that processes a plurality of substrates at a time is described. The present invention is not limited to the above-described embodiments, and is also applicable to a case where a film is formed using a sheet-by-sheet substrate processing apparatus that processes one or a plurality of substrates at a time, for example. In the above-described embodiments, an example of forming a film using a substrate processing apparatus having a hot wall type processing furnace is described. The present invention is not limited to the above-described embodiments, and is also applicable to a case where a film is formed using a substrate processing apparatus having a cold wall type processing furnace.
Even when these substrate processing apparatuses are used, substrate processing can be performed in the same sequence and under the same processing conditions as those in the above-described embodiment, and the same effects as those in the above-described embodiment can be obtained. That is, the present invention is applicable to a case where a substrate processing apparatus configured to discharge a source gas supplied from a first supply unit to a substrate from an exhaust port disposed at least at a position facing the first supply unit with the substrate interposed therebetween in a plan view is used. The present invention is applicable to a case where a substrate processing apparatus configured to supply a raw material gas and an inert gas to a substrate from a side of the substrate and supply a reaction gas to the substrate from a side of the substrate is used.
In addition, the above embodiments can be used in combination as appropriate. The processing procedure and the processing conditions in this case may be the same as those in the above-described embodiment, for example.
[ examples ] A method for producing a compound
As an example, a SiN film was formed on a wafer by the film formation sequence shown in fig. 5 using the substrate processing apparatus shown in fig. 1. In the DCS gas supply step, N is supplied from the first supply part2The gas is supplied together with DCS gas, and the pressure in the processing chamber at this time is made to be NH3The pressure in the processing chamber in the gas supply step is high. The process condition in the DCS gas supply step is set to a condition that the amount of decomposition of DCS gas in the first supply unit is greater than the amount of decomposition of DCS gas in the process chamber. The other processing conditions are predetermined conditions within the processing condition range described in the second embodiment.
As comparative example 1, the substrate processing apparatus shown in fig. 1 was used, and the step of supplying DCS gas from the first supply unit to the wafer and the step of supplying NH from the second supply unit to the wafer were alternately repeated3And a step of gas, thereby forming a SiN film on the wafer. In DCS gas supplyIn the step, N is supplied from a first supply part2The gas is supplied together with DCS gas, and the pressure in the processing chamber at this time is set to be NH3The pressure in the processing chamber in the gas supply step is small. The process condition in the DCS gas supply step is set to a predetermined condition that the amount of decomposition of DCS gas in the first supply unit is equal to or less than the amount of decomposition of DCS gas in the process chamber. N supplied from the first supply part together with DCS gas2The flow rate of the gas was N supplied from the first supply unit together with DCS gas in the example2The flow rate of the gas is 1/5-1/10. Other processing steps and processing conditions were the same as those in the examples.
As comparative example 2, the substrate processing apparatus shown in fig. 1 was used, and the step of supplying DCS gas from the first supply unit to the wafer and the step of supplying NH from the second supply unit to the wafer were alternately repeated3And a step of gas, thereby forming a SiN film on the wafer. In the DCS gas supply step, the supply of N from the first supply part is not performed2Gas, and the pressure in the processing chamber is set to be NH3The pressure in the processing chamber in the gas supply step is small. The process condition in the DCS gas supply step is set to a predetermined condition that the amount of decomposition of DCS gas in the first supply unit is smaller than the amount of decomposition of DCS gas in the process chamber. Other processing steps and processing conditions were the same as those in the examples.
Next, the in-plane refractive index uniformity (r.i. range) and the in-plane film thickness uniformity (WiW) of the SiN films formed in example 1 and comparative examples 1 and 2 were measured. The measurement results are shown in fig. 8. Both r.i.range and WiW [% ] mean that the smaller the value, the higher the in-wafer uniformity (uniformity).
As shown in fig. 8, it is understood that the values of r.i. range and WiW are smaller in example 1 than in comparative examples 1 and 2. That is, it was found that by performing the DCS gas supply step under the condition that the amount of decomposition of DCS gas in the first supply unit is larger than the amount of decomposition of DCS gas in the process chamber, the uniformity of the in-plane refractive index and the uniformity of the in-plane film thickness of the SiN film formed on the wafer can be improved.

Claims (21)

1. A method for manufacturing a semiconductor device, characterized in that,
there is a step of forming a film on a substrate by performing cycles for a predetermined number of times,
the above cycles are performed non-simultaneously:
(a) supplying a source gas from a first supply unit to the substrate in the processing chamber; and
(b) supplying a reaction gas from a second supply unit to the substrate in the processing chamber,
in the step (a), the raw material gas is decomposed in the first supply unit and the processing chamber to generate an intermediate, and the intermediate is supplied to the substrate, and in this case, the decomposition amount of the raw material gas in the first supply unit is set to be larger than the decomposition amount of the raw material gas in the processing chamber.
2. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the decomposition rate of the source gas in the first supply unit is set to be higher than the decomposition rate of the source gas in the processing chamber.
3. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the decomposition rate of the source gas in the first supply unit is set to be higher than the decomposition rate of the source gas in the processing chamber.
4. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the amount of the intermediate produced in the first supply unit is set to be larger than the amount of the intermediate produced in the processing chamber.
5. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the rate of production of the intermediate in the first supply unit is set to be higher than the rate of production of the intermediate in the processing chamber.
6. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the intermediate production rate in the first supply unit is set to be higher than the intermediate production rate in the processing chamber.
7. The method for manufacturing a semiconductor device according to claim 1,
the opening area of the gas ejection port provided in the first supply portion is set to an opening area (a) in which the amount of decomposition of the raw material gas in the first supply portion is larger than the amount of decomposition of the raw material gas in the processing chamber.
8. The method for manufacturing a semiconductor device according to claim 1,
the opening area of the gas ejection port provided in the first supply portion is set to be equal to or smaller than the opening area of the gas ejection port provided in the second supply portion.
9. The method for manufacturing a semiconductor device according to claim 1,
the opening area of the gas ejection port provided in the first supply portion is made smaller than the opening area of the gas ejection port provided in the second supply portion.
10. The method for manufacturing a semiconductor device according to claim 1,
and a third supply unit different from the first supply unit and the second supply unit,
the second supply part and the third supply part are arranged in a manner of clamping the first supply part from two sides,
in the step (a), an inert gas is supplied from each of the second supply part and the third supply part,
the opening area of the gas ejection port provided in the first supply portion is set to be equal to or smaller than the opening area of the gas ejection port provided in each of the second supply portion and the third supply portion.
11. The method for manufacturing a semiconductor device according to claim 1,
and a third supply unit different from the first supply unit and the second supply unit,
the second supply part and the third supply part are arranged in a manner of clamping the first supply part from two sides,
in the step (a), an inert gas is supplied from each of the second supply part and the third supply part,
the opening area of the gas ejection port provided in the first supply portion is made smaller than the opening area of the gas ejection port provided in each of the second supply portion and the third supply portion.
12. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), an inert gas is supplied from the first supply unit to the substrate,
the flow rate of the inert gas supplied from the first supply unit is set to be larger than the flow rate of the raw material gas supplied from the first supply unit.
13. The method for manufacturing a semiconductor device according to claim 12,
in the step (a), an inert gas is supplied from the second supply part,
the flow rate of the inert gas supplied from the first supply unit is made larger than the flow rate of the inert gas supplied from the second supply unit.
14. The method for manufacturing a semiconductor device according to claim 12,
and a third supply unit different from the first supply unit and the second supply unit,
the second supply part and the third supply part are arranged in a manner of clamping the first supply part from two sides,
in the step (a), an inert gas is supplied from each of the second supply part and the third supply part,
the flow rate of the inert gas supplied from the first supply unit is made larger than the flow rate of the inert gas supplied from each of the second supply unit and the third supply unit.
15. The method for manufacturing a semiconductor device according to claim 12,
and a third supply unit different from the first supply unit and the second supply unit,
the second supply part and the third supply part are arranged in a manner of clamping the first supply part from two sides,
in the step (a), an inert gas is supplied from each of the second supply part and the third supply part,
the flow rate of the inert gas supplied from the first supply unit is made larger than the total flow rate of the inert gas supplied from each of the second supply unit and the third supply unit.
16. The method for manufacturing a semiconductor device according to claim 1,
setting the pressure in the processing chamber in (a) to be equal to or higher than the pressure in the processing chamber in (b).
17. The method for manufacturing a semiconductor device according to claim 1,
the pressure in the processing chamber in (a) is set to be higher than the pressure in the processing chamber in (b).
18. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the source gas supplied to the substrate is discharged from a gas discharge port disposed at least at a position facing the first supply portion with the substrate interposed therebetween in a plan view.
19. The method for manufacturing a semiconductor device according to claim 1,
in the step (a), the raw material gas and the inert gas are supplied to the substrate from a side of the substrate,
in the step (b), the reaction gas is supplied to the substrate from a side of the substrate.
20. A substrate processing apparatus includes:
a processing chamber for processing a substrate;
a source gas supply system configured to supply a source gas from a first supply unit to the substrate in the processing chamber;
a reaction gas supply system for supplying a reaction gas from a second supply unit to the substrate in the processing chamber;
a decomposition unit that decomposes the source gas in the first supply unit and the processing chamber; and
and a control unit configured to control the raw material gas supply system, the reaction gas supply system, and the decomposition unit to perform a process of forming a film on the substrate by performing a predetermined number of cycles of non-simultaneous (a) a process of supplying the raw material gas from the first supply unit to the substrate in the processing chamber and (b) a process of supplying the reaction gas from the second supply unit to the substrate in the processing chamber, wherein in (a), the raw material gas is decomposed in the first supply unit and the processing chamber to generate an intermediate, and the intermediate is supplied to the substrate, and at this time, a decomposition amount of the raw material gas in the first supply unit is set to be larger than a decomposition amount of the raw material gas in the processing chamber.
21. A computer-readable storage medium storing a program for causing a substrate processing apparatus to execute, by a computer, the steps of:
a step of forming a film on a substrate by performing a predetermined number of cycles of (a) supplying a raw material gas from a first supply unit to the substrate in a processing chamber of the substrate processing apparatus and (b) supplying a reaction gas from a second supply unit to the substrate in the processing chamber, non-simultaneously; and
in the step (a), the raw material gas is decomposed in the first supply unit and the processing chamber to generate an intermediate, and the intermediate is supplied to the substrate, and in this case, the decomposition amount of the raw material gas in the first supply unit is set to be larger than the decomposition amount of the raw material gas in the processing chamber.
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